中国药业2017,Vol.26Issue(9):29-32,4.DOI:10.3969/j.issn.1006-4931.2017.09.009
顶空气相色谱法检测血塞通分散片中有机溶剂残留量
Determination of Residual Organic Solvents in Xuesaitong Dispersible Tablets by Headspace Gas Chromatography
李培 1董青1
作者信息
- 1. 山东省聊城市食品药品检验检测中心,山东聊城 252000
- 折叠
摘要
Abstract
Objective To establish the headspace gas chromatography method for determination of six residual organic solvent in Xue-saitong Dispersible Tablets. Methods The chromatographic column adopted HP-INNOWAX capillary column with polyethylene glycol as stationary phase ( 30 m × 0. 32 mm. 0. 25 μm ) . and the FID was used. The column temperature was programmed by heating: the initial temperature was 60 ℃. keep for 1 min. then the temperature was increased to 100 ℃ at 5 ℃ /min. keep for 13 min. and then increase to 200 ℃ at 20 ℃ /min. keep for 2 min. The inlet temperature was 240 ℃. the detector temperature was 300 ℃. the carrier gas was nitrogen. the flow rate was 2. 5 mL/min. Headspace sampling was adopted. headspace equilibrium temperature was 70 ℃. and equilibrium time was 30 min. Results The concentration linear range of hexane. toluene. p-xylene. o-xylene. styrene. 1. 2-diethylbenzene were 1. 014-16. 224. 1. 060-16. 960. 1. 610-18. 576. 1. 169-18. 704. 0. 985-15. 760. 1. 129-18. 064 g/mL. respectively. and the relative conditions of r were 0. 9996. 0. 9999. 0. 9999. 0. 9996. 0. 9994. 0. 9992. respectively. The recovery rates were 97. 14% -98. 73%( n=9 ) . The theoretical plates were larger than 10000. and the separation degree of adjacent peaks was above 2. 0. Conclusion The method has simple sample processing. accurate detection. high sensitivity and good reproducibility. and excludes the interference of excipi-ents. which can be used as an investigation method for the determination of residual organic solvents in Xuesaitong Dispersible Tablets.关键词
顶空/气相色谱法/血塞通分散片/有机溶剂残留Key words
headspace/gas chromatography/Xuesaitong Dispersible Tablets/residue organic solvent分类
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李培,董青..顶空气相色谱法检测血塞通分散片中有机溶剂残留量[J].中国药业,2017,26(9):29-32,4.